Water → 2-Aminocarbonyloxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(beta-ethoxyethoxy)carbonyl-1,4-dihydropyridine

HRID 1995439ノート

反応式

HRID 1995439 の反応式
[OH:1][CH2:2][C:3]1[NH:4][C:5]([CH3:31])=[C:6]([C:23]([O:25][CH2:26][CH2:27][O:28][CH2:29][CH3:30])=[O:24])[CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].ClS([N:36]=[C:37]=[O:38])(=O)=O.O.C(OC(C)C)(C)C.CCCCCC>C1C=CC=CC=1>[NH2:36][C:37]([O:1][CH2:2][C:3]1[NH:4][C:5]([CH3:31])=[C:6]([C:23]([O:25][CH2:26][CH2:27][O:28][CH2:29][CH3:30])=[O:24])[CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:38]

参加物

6

反応物 4

HCID 962WaterHCID 70918Chlorosulfonyl isocyanateHCID 130921522-Ethoxyethyl 2-methyl-4-(3-nitrophenyl)-5-ethoxycarbonyl-6-hydroxymethyl-1,4-dihydropyridine-3-carboxylateHCID 21881879Diisopropylether hexane

生成物 1

HCID 130921162-Aminocarbonyloxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(beta-ethoxyethoxy)carbonyl-1,4-dihydropyridine収率 62.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

2-Hydroxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(β-ethoxyethoxy)carbonyl-1,4-dihydropyridine (420 mg) was dissolved in benzene (20 ml), chlorosulfonyl isocyanate (0.2 ml) was added thereto, and the mixture was reacted under stirring at room temperature for 30 minutes. Water (10 ml) was added to the reaction mixture under cooling, and the mixture was stirred at room temperature for 30 minutes for hydrolysis. The reaction mixture thus obtained was extracted with ethyl acetate, and the extracted solution was washed with water, dried and then concentrated under reduced pressure. The residue was recrystallized from diisopropyl ether/hexane, whereupon crystals (290 mg, yield: 62.6%) were obtained.

後処理

  1. customthe mixture was reacted
  2. temperatureunder cooling
  3. stirringthe mixture was stirred at room temperature for 30 minutes for hydrolysis
  4. customThe reaction mixture thus obtained
  5. extractionwas extracted with ethyl acetate
  6. washthe extracted solution was washed with water
  7. customdried
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-02c72069074045b18b498c1608cf0e2b
出典データセット
uspto-grants-1983_09
特許番号
US04404378

反応ノート

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